CN107185546A - A kind of bismuth ferrite graphene oxide composite material preparation method - Google Patents

A kind of bismuth ferrite graphene oxide composite material preparation method Download PDF

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CN107185546A
CN107185546A CN201710325049.8A CN201710325049A CN107185546A CN 107185546 A CN107185546 A CN 107185546A CN 201710325049 A CN201710325049 A CN 201710325049A CN 107185546 A CN107185546 A CN 107185546A
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bismuth ferrite
graphene oxide
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ice bath
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吴化平
王有岩
徐振雄
刘爱萍
张征
丁浩
李吉泉
鲁聪达
令欢
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Zhejiang University of Technology ZJUT
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    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
    • B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
    • B01J23/76—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
    • B01J23/84—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36 with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
    • B01J23/843—Arsenic, antimony or bismuth
    • B01J23/8437—Bismuth
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J35/00—Catalysts, in general, characterised by their form or physical properties
    • B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
    • B01J35/39—Photocatalytic properties

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Abstract

The invention discloses a kind of bismuth ferrite graphene oxide composite material preparation method, comprise the following steps：Step（1）Prepare graphene oxide solution, step（2）Prepare bismuth ferrite powder, step（3）Prepare bismuth ferrite powder and three-dimensional graphene oxide compound.The bismuth ferrite graphene oxide compound prepared according to preparation method of the present invention, bismuth ferrite is sub-micron cube powder, mutually it is bonded together with the shape of small cubic block, the three-dimensional graphene oxide of film-form is coated on the surface of bismuth ferrite cube, spontaneous polarization inside bismuth ferrite cube powder can pull open photo-generate electron-hole pair, so as to reduce its recombination probability, and then improve photocatalytic activity and electricity conversion, bismuth ferrite sub-micron cube powder can increase the area of catalytic surface with three-dimensional graphene oxide compound, three-dimensional surface of graphene oxide can form more electron channels, be conducive to the progress of catalytic reaction, so as to improve photocatalytic activity.

Description

一种铁酸铋-氧化石墨烯复合材料制备方法A kind of preparation method of bismuth ferrite-graphene oxide composite material

技术领域technical field

本发明涉及一种可用作光催化活性的铁酸铋-氧化石墨烯复合材料制备方法。The invention relates to a method for preparing a bismuth ferrite-graphene oxide composite material that can be used as photocatalytic activity.

背景技术Background technique

光催化是在一定波长光照条件下，半导体材料发生光生载流子的分离，然后光生电子和空穴在与离子或分子结合生成具有氧化性或还原性的活性自由基，这种活性自由基能将有机物大分子降解为二氧化碳或其他小分子有机物以及水，在反应过程中这种半导体材料也就是光催化剂本身不发生变化。光催化技术是一种新型纳米环境净化技术，在有光照的条件下，光触媒可持续不断地净化室内外空气，消毒杀菌，用于建筑物外墙又可产生自清洁效果，光催化技术作为一种高效、安全的环境友好型环境净化技术，对室内空气质量的改善已得到国际学术界的认可，光催化技术已广泛应用在无机污染物废水处理、有机化合物的处理、抗菌处理以及空气的净化等方面。Photocatalysis is the separation of photogenerated carriers in semiconductor materials under the condition of light of a certain wavelength, and then the photogenerated electrons and holes combine with ions or molecules to generate oxidative or reductive active free radicals. The organic macromolecules are degraded into carbon dioxide or other small molecular organic substances and water, and the semiconductor material, that is, the photocatalyst itself, does not change during the reaction. Photocatalytic technology is a new type of nano-environment purification technology. Under the condition of light, photocatalyst can continuously purify indoor and outdoor air, disinfect and sterilize, and can produce self-cleaning effect when used on the exterior wall of buildings. Photocatalytic technology is a An efficient and safe environment-friendly environmental purification technology, the improvement of indoor air quality has been recognized by the international academic community, photocatalytic technology has been widely used in inorganic pollutant wastewater treatment, organic compound treatment, antibacterial treatment and air purification etc.

目前，提高半导体光催化活性的方法主要有离子掺杂、表面贵金属沉积、半导体的光敏化、改变光催化剂的表面形貌等，但目前所用的方法存在很多问题，性能有待提升，从而制备出具有高的光催化活性的催化剂是十分必要的，针对此现状，本发明提出了一种可提高光催化活性的铁酸铋-氧化石墨烯半导体复合材料制备方法。At present, the methods for improving the photocatalytic activity of semiconductors mainly include ion doping, surface precious metal deposition, photosensitization of semiconductors, and changing the surface morphology of photocatalysts, etc., but there are many problems in the current methods, and the performance needs to be improved. Catalysts with high photocatalytic activity are very necessary. Aiming at the present situation, the present invention proposes a method for preparing a bismuth ferrite-graphene oxide semiconductor composite material that can improve photocatalytic activity.

发明内容Contents of the invention

本发明针对目前市场上没有一种简单有效的制备方法来制备具有高的光催化活性的催化剂的问题，提出了一种便于操作，可靠高效的铁酸铋-氧化石墨烯复合材料制备方法。Aiming at the problem that there is no simple and effective preparation method on the market to prepare a catalyst with high photocatalytic activity, the present invention proposes an easy-to-operate, reliable and efficient preparation method of bismuth ferrite-graphene oxide composite material.

本发明的技术方案是这样的：一种铁酸铋-氧化石墨烯复合材料制备方法，包括以下步骤：The technical scheme of the present invention is such: a kind of bismuth ferrite-graphene oxide composite material preparation method comprises the following steps:

步骤（1）制备氧化石墨烯溶液：称取一定量的石墨粉、硝酸钠和高锰酸钾，其质量比为2:1:4；将石墨粉与硝酸钠放入烧杯中，并在烧杯中逐滴加入浓硫酸，滴加量为石墨粉、硝酸钠之和的15~20倍（质量份），保持在5℃以下进行冰浴处理，在冰浴开始时、15min时和30min时各加入所述高锰酸钾的1/3，加完后保持5~10℃进行低温反应，反应时间为90min；而后保持35~40℃进行中温反应，反应为时间30min；再在5℃以下进行冰浴处理，冰浴时间为20min，在冰浴过程中加入常温的去离子水，加入量为初始石墨粉的20~30倍（质量份）；冰浴结束后加入初始石墨粉的10~15倍（质量份）的去离子水和初始石墨粉的1~2倍（质量份）的双氧水，在80~90℃进行高温反应，反应时间为30min；高温反应时反应终止后进行离心操作，离心转速为2000r/min，每次离心时间为10min，共离心处理6次，使溶液变粘稠，然后离心转速提高到8000r/min，每次离心时间为10min，共离心处理3次，继续将离心转速提高到10000r/min，每次离心时间为10min，离心处理一次后进行超声处理，超声处理后再次离心，离心转速为4000r/min，每次离心时间为10min，共处理2次，最后得到氧化石墨烯溶液；Step (1) Prepare graphene oxide solution: weigh a certain amount of graphite powder, sodium nitrate and potassium permanganate, the mass ratio of which is 2:1:4; put graphite powder and sodium nitrate into a beaker, and Concentrated sulfuric acid was added dropwise to the medium, and the amount added was 15 to 20 times (parts by mass) of the sum of graphite powder and sodium nitrate, and the temperature was kept below 5°C for ice bath treatment. Add 1/3 of the potassium permanganate, after adding, keep 5~10°C for low temperature reaction, the reaction time is 90min; then keep 35~40°C for medium temperature reaction, the reaction time is 30min; Ice bath treatment, the ice bath time is 20min, add deionized water at room temperature during the ice bath, the addition amount is 20~30 times (mass parts) of the initial graphite powder; after the ice bath, add 10~15 times the original graphite powder Times (parts by mass) of deionized water and 1-2 times (parts by mass) of hydrogen peroxide of the initial graphite powder, high-temperature reaction at 80-90°C, the reaction time is 30min; The rotating speed is 2000r/min, each centrifugation time is 10min, and centrifugation is processed 6 times in total to make the solution viscous, then the centrifugation speed is increased to 8000r/min, each centrifugation time is 10min, centrifugation is 3 times in total, and the centrifugation is continued. The rotation speed was increased to 10000r/min, and the centrifugation time was 10min each time. Ultrasonic treatment was performed after one centrifugation treatment. Graphene solution;

步骤（2）制备铁酸铋粉末：首先称量Bi(NO3)3·5H2O与Fe(NO3)3·9H2O 溶于去离子水中，三者摩尔比为1:1：50，搅拌直到晶体全部溶解；然后制备2mol/L的NaOH溶液，在搅拌下缓慢加入前述含有Bi3+、Fe3+的混合溶液中，直至pH大于13.5，此时产生大量橘黄色的沉淀，快速搅拌40min以保证沉淀均匀混合；加入体积浓度为30%的双氧水，加入量为前述去离子水的5~10%（体积比），趁热放入反应釜中，水热温度200℃，水热时间72h；结束后，将所得溶液进行离心清洗至中性，放入鼓风干燥箱中进行干燥，得到铁酸铋亚微米立方粉末；Step (2) Preparation of bismuth ferrite powder: first weigh Bi(NO 3 ) 3 5H 2 O and Fe(NO 3 ) 3 9H 2 O and dissolve them in deionized water, the molar ratio of the three is 1:1:50 , stir until the crystals are completely dissolved; then prepare a 2mol/L NaOH solution, and slowly add it into the aforementioned mixed solution containing Bi 3+ and Fe 3+ under stirring until the pH is greater than 13.5. Stir for 40 minutes to ensure that the precipitate is evenly mixed; add hydrogen peroxide with a volume concentration of 30%, and the amount added is 5-10% (volume ratio) of the aforementioned deionized water, and put it into the reaction kettle while it is hot. The time is 72 hours; after the end, the obtained solution is centrifugally cleaned to neutrality, and put into a blast drying oven for drying to obtain submicron cubic powder of bismuth ferrite;

步骤（3）制备铁酸铋粉末与三维氧化石墨烯复合物：取步骤（1）得到的氧化石墨烯溶液，加2~4倍水（体积比）稀释为稀溶液，加入步骤（2）得到的铁酸铋粉末，加入的量为每1克铁酸铋粉末对应于400~500ml稀溶液，超声搅拌均匀；将所得混合液移入反应釜内进行水热反应，水热温度160℃，水热时间6h；最后将所得三维复合物进行透析，放入冷冻干燥机中干燥，得到铁酸铋-氧化石墨烯复合材料。Step (3) Preparation of bismuth ferrite powder and three-dimensional graphene oxide composite: take the graphene oxide solution obtained in step (1), add 2 to 4 times of water (volume ratio) to dilute it into a dilute solution, add step (2) to obtain Bismuth ferrite powder, the amount added is 400~500ml dilute solution per 1 gram of bismuth ferrite powder, and ultrasonically stirred evenly; move the resulting mixed solution into the reaction kettle for hydrothermal reaction, the hydrothermal temperature is 160°C, the hydrothermal The time is 6 hours; finally, the obtained three-dimensional composite is dialyzed and dried in a freeze dryer to obtain a bismuth ferrite-graphene oxide composite material.

根据本发明所述的制备方法制备的铁酸铋-氧化石墨烯复合物，铁酸铋为亚微米立方粉末，以小立方块的形状相互粘结在一起，薄膜状的三维氧化石墨烯包覆在铁酸铋立方的表面，铁酸铋立方粉末内部的自发极化可拉开光生电子-空穴对，从而减少其复合几率，进而提高光催化活性和光电转化效率，铁酸铋亚微米立方粉末与三维氧化石墨烯复合物能增加催化表面的面积，三维氧化石墨烯表面可以形成更多的电子通道，有利于催化反应的进行，从而提高光催化活性。According to the bismuth ferrite-graphene oxide composite prepared by the preparation method of the present invention, the bismuth ferrite is a submicron cubic powder, which is bonded together in the shape of small cubes, and is covered with film-like three-dimensional graphene oxide. On the surface of bismuth ferrite cubic, the spontaneous polarization inside the bismuth ferrite cubic powder can pull apart photogenerated electron-hole pairs, thereby reducing their recombination probability, thereby improving photocatalytic activity and photoelectric conversion efficiency, bismuth ferrite submicron cubic The composite of powder and three-dimensional graphene oxide can increase the area of the catalytic surface, and more electron channels can be formed on the surface of three-dimensional graphene oxide, which is conducive to the progress of the catalytic reaction, thereby improving the photocatalytic activity.

本发明的有益效果是：1）铁酸铋亚微米立方晶体内部的自发极化可拉开光生电子-空穴对，可以提高光催化活性。The beneficial effects of the invention are as follows: 1) The spontaneous polarization inside the bismuth ferrite submicron cubic crystal can pull apart the photogenerated electron-hole pairs, and can improve the photocatalytic activity.

2）三维氧化石墨烯包裹在铁酸铋亚微米立方表面，大大增加了催化表面的面积，而且三维氧化石墨烯表面可以形成更多的电子通道，从而提高光催化活性。2) The three-dimensional graphene oxide is wrapped on the submicron cubic surface of bismuth ferrite, which greatly increases the area of the catalytic surface, and the surface of the three-dimensional graphene oxide can form more electron channels, thereby improving the photocatalytic activity.

3）制备方法可靠，便于操作。3) The preparation method is reliable and easy to operate.

具体实施方式detailed description

下面结合实施例进一步说明本发明。Below in conjunction with embodiment further illustrate the present invention.

实施例1包括以下步骤：Embodiment 1 comprises the following steps:

步骤（1）制备氧化石墨烯溶液：称取一定量的石墨粉、硝酸钠和高锰酸钾，其质量比为2:1:4；将石墨粉与硝酸钠放入烧杯中，并在烧杯中逐滴加入浓硫酸，滴加量为石墨粉、硝酸钠之和的15~20倍（质量份），保持在5℃以下进行冰浴处理，在冰浴开始时、15min时和30min时各加入所述高锰酸钾的1/3，加完后保持5~10℃进行低温反应，反应时间为90min；而后保持35~40℃进行中温反应，反应为时间30min；再在5℃以下进行冰浴处理，冰浴时间为20min，在冰浴过程中加入常温的去离子水，加入量为初始石墨粉的20~30倍（质量份）；冰浴结束后加入初始石墨粉的10~15倍（质量份）的去离子水和初始石墨粉的1~2倍（质量份）的双氧水，在80~90℃进行高温反应，反应时间为30min；高温反应时反应终止后进行离心操作，离心转速为2000r/min，每次离心时间为10min，共离心处理6次，使溶液变粘稠，然后离心转速提高到8000r/min，每次离心时间为10min，共离心处理3次，继续将离心转速提高到10000r/min，每次离心时间为10min，离心处理一次后进行超声处理，超声处理后再次离心，离心转速为4000r/min，每次离心时间为10min，共处理2次，最后得到氧化石墨烯溶液；Step (1) Prepare graphene oxide solution: weigh a certain amount of graphite powder, sodium nitrate and potassium permanganate, the mass ratio of which is 2:1:4; put graphite powder and sodium nitrate into a beaker, and Concentrated sulfuric acid was added dropwise to the medium, and the amount added was 15 to 20 times (parts by mass) of the sum of graphite powder and sodium nitrate, and the temperature was kept below 5°C for ice bath treatment. Add 1/3 of the potassium permanganate, after adding, keep 5~10°C for low temperature reaction, the reaction time is 90min; then keep 35~40°C for medium temperature reaction, the reaction time is 30min; Ice bath treatment, the ice bath time is 20min, add deionized water at room temperature during the ice bath, the addition amount is 20~30 times (mass parts) of the initial graphite powder; after the ice bath, add 10~15 times the original graphite powder Times (parts by mass) of deionized water and 1-2 times (parts by mass) of hydrogen peroxide of the initial graphite powder, high-temperature reaction at 80-90°C, the reaction time is 30min; The rotating speed is 2000r/min, each centrifugation time is 10min, and centrifugation is processed 6 times in total to make the solution viscous, then the centrifugation speed is increased to 8000r/min, each centrifugation time is 10min, centrifugation is 3 times in total, and the centrifugation is continued. The rotation speed was increased to 10000r/min, and the centrifugation time was 10min each time. Ultrasonic treatment was performed after one centrifugation treatment. Graphene solution;

步骤（2）制备铁酸铋粉末：首先称量Bi(NO3)3·5H2O与Fe(NO3)3·9H2O 溶于去离子水中，三者摩尔比为1:1：50，搅拌直到晶体全部溶解；然后制备2mol/L的NaOH溶液，在搅拌下缓慢加入前述含有Bi3+、Fe3+的混合溶液中，直至pH大于13.5，此时产生大量橘黄色的沉淀，快速搅拌40min以保证沉淀均匀混合；加入体积浓度为30%的双氧水，加入量为前述去离子水的5~10%（体积比），趁热放入反应釜中，水热温度200℃，水热时间72h；结束后，将所得溶液进行离心清洗至中性，放入鼓风干燥箱中进行干燥，得到铁酸铋亚微米立方粉末；Step (2) Preparation of bismuth ferrite powder: first weigh Bi(NO 3 ) 3 5H 2 O and Fe(NO 3 ) 3 9H 2 O and dissolve them in deionized water, the molar ratio of the three is 1:1:50 , stir until the crystals are completely dissolved; then prepare a 2mol/L NaOH solution, and slowly add it into the aforementioned mixed solution containing Bi 3+ and Fe 3+ under stirring until the pH is greater than 13.5. Stir for 40 minutes to ensure that the precipitate is evenly mixed; add hydrogen peroxide with a volume concentration of 30%, and the amount added is 5-10% (volume ratio) of the aforementioned deionized water, and put it into the reaction kettle while it is hot. The time is 72 hours; after the end, the obtained solution is centrifugally cleaned to neutrality, and put into a blast drying oven for drying to obtain submicron cubic powder of bismuth ferrite;

步骤（3）制备铁酸铋粉末与三维氧化石墨烯复合物：取步骤（1）得到的氧化石墨烯溶液，加2~4倍水（体积比）稀释为稀溶液，加入步骤（2）得到的铁酸铋粉末，加入的量为每1克铁酸铋粉末对应于400~500ml稀溶液，超声搅拌均匀；将所得混合液移入反应釜内进行水热反应，水热温度160℃，水热时间6h；最后将所得三维复合物进行透析，放入冷冻干燥机中干燥，得到铁酸铋-氧化石墨烯复合材料。Step (3) Preparation of bismuth ferrite powder and three-dimensional graphene oxide composite: take the graphene oxide solution obtained in step (1), add 2 to 4 times of water (volume ratio) to dilute it into a dilute solution, add step (2) to obtain Bismuth ferrite powder, the amount added is 400~500ml dilute solution per 1 gram of bismuth ferrite powder, and ultrasonically stirred evenly; move the resulting mixed solution into the reaction kettle for hydrothermal reaction, the hydrothermal temperature is 160°C, the hydrothermal The time is 6 hours; finally, the obtained three-dimensional composite is dialyzed and dried in a freeze dryer to obtain a bismuth ferrite-graphene oxide composite material.

本说明书实施例所述的内容仅仅是对发明构想的实现形式的列举，本发明的保护范围不应当被视为仅限于实施例所陈述的具体形式，本发明的保护范围也包括本领域技术人员根据本发明构思所能够想到的等同技术手段。The content described in the embodiments of this specification is only an enumeration of the realization forms of the inventive concept. The protection scope of the present invention should not be regarded as limited to the specific forms stated in the embodiments. The protection scope of the present invention also includes those skilled in the art. Equivalent technical means conceivable according to the concept of the present invention.

Claims (1)

1. a kind of bismuth ferrite-graphene oxide composite material preparation method, comprises the following steps：
Step（1）Prepare graphene oxide solution：A certain amount of graphite powder, sodium nitrate and potassium permanganate are weighed, its mass ratio is 2:1:4；Graphite powder and sodium nitrate are put into beaker, and the concentrated sulfuric acid is added dropwise in beaker, dripping quantity is graphite powder, nitric acid 15 ~ 20 times of sodium sum（Mass parts）, less than 5 DEG C progress ice bath processing are maintained at, when when ice bath starts, 15min and 30min When respectively add the 1/3 of the potassium permanganate, after adding keep 5 ~ 10 DEG C progress low-temp reactions, the reaction time is 90min；Then protect Hold 35 ~ 40 DEG C and carry out middle temperature reaction, react for time 30min；Ice bath processing is carried out below 5 DEG C again, the ice bath time is 20min, adds the deionized water of normal temperature during ice bath, and addition is 20 ~ 30 times of starting graphite powder（Mass parts）；Ice bath 10 ~ 15 times of starting graphite powder are added after end（Mass parts）Deionized water and 1 ~ 2 times of starting graphite powder（Mass parts）'s Hydrogen peroxide, carries out pyroreaction, the reaction time is 30min at 80 ~ 90 DEG C；Centrifugation behaviour is carried out during pyroreaction after reaction terminating Make, centrifugal rotational speed is 2000r/min, each centrifugation time is 10min, and centrifugal treating 6 times, becomes viscous solution, Ran Houli altogether Heart rotating speed brings up to 8000r/min, and each centrifugation time is 10min, altogether centrifugal treating 3 times, and continuation brings up to centrifugal rotational speed 10000r/min, each centrifugation time be 10min, centrifugal treating once carry out afterwards it is ultrasonically treated, it is ultrasonically treated after centrifuge again, Centrifugal rotational speed is 4000r/min, and each centrifugation time is 10min, and coprocessing 2 times finally obtains graphene oxide solution；
Step（2）Prepare bismuth ferrite powder：Bi (NO are weighed first3)3·5H2O and Fe (NO3)3·9H2O is dissolved in deionized water In, three's mol ratio is 1:1：50, stirring is all dissolved until crystal；Then 2mol/L NaOH solution is prepared, under agitation It is slowly added to foregoing containing Bi3+、Fe3+Mixed solution in, until pH be more than 13.5, now produce the precipitation of a large amount of crocus, It is quick to stir 40min to ensure to precipitate uniform mixing；The hydrogen peroxide that volumetric concentration is 30% is added, addition is foregoing deionization The 5 ~ 10% of water（Volume ratio）, it is put into while hot in reactor, 200 DEG C of hydrothermal temperature, hydro-thermal time 72h；It is after end, gained is molten Liquid carries out eccentric cleaning to neutrality, is put into air dry oven and is dried, obtains bismuth ferrite sub-micron cube powder；
Step（3）Prepare bismuth ferrite powder and three-dimensional graphene oxide compound：Take step（1）Obtained graphene oxide is molten Liquid, plus 2 ~ 4 times of water（Volume ratio）Weak solution is diluted to, step is added（2）Obtained bismuth ferrite powder, the amount of addition is every 1 gram Bismuth ferrite powder corresponds to 400 ~ 500ml weak solutions, and ultrasonic agitation is uniform；Gained mixed liquor is moved into reactor and carries out hydro-thermal Reaction, 160 DEG C of hydrothermal temperature, hydro-thermal time 6h；Finally gained three-dimensional composite is dialysed, is put into freeze drier and does It is dry, obtain bismuth ferrite-graphene oxide composite material.
CN201710325049.8A 2017-05-10 2017-05-10 A kind of bismuth ferrite graphene oxide composite material preparation method Pending CN107185546A (en)

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CN111111683A (en) * 2019-12-31 2020-05-08 西南石油大学 A kind of composite photocatalyst and preparation method thereof
CN112495364A (en) * 2020-12-15 2021-03-16 陕西科技大学 Bi12SiO20-Bi2O2SiO3Preparation method of/rGO photocatalyst
CN114669301A (en) * 2022-04-19 2022-06-28 华北理工大学 Three-dimensional graphene gel composite material and preparation and application methods thereof
CN118929770A (en) * 2024-10-11 2024-11-12 内蒙古工业大学 Graphene oxide coated bismuth ferrite anode material and preparation method thereof and negative electrode sheet

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Application publication date: 20170922